KR20150086037A - Method of manufacturing graphene encapsulation film and method of organic electronic device having the same. - Google Patents

Abstract

The present invention relates to a method for manufacturing a graphene encapsulation film and a method for manufacturing an organic electronic device having the same. In the method for manufacturing a graphene encapsulation film; a first graphene layer is formed on a base substrate and a first organic film is connected to a target substrate; and the first graphene layer is mechanically exfoliated to transfer the first graphene layer to the first organic film.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method of manufacturing a graphene sealing film and a method of manufacturing the same.

The present invention relates to a method of manufacturing a sealing film using graphene, and more particularly, to a method of manufacturing a graphene sealing film including a plurality of graphene layers and an organic film alternately laminated to each other, And a manufacturing method thereof.

Graphene refers to a planar two-dimensional carbon structure that forms sp2 bonds, and is a material with high physical and chemical stability. Graphene is a hexagonal lattice structure and is a very effective material that can prevent gas and moisture permeation. Also, it has a thickness corresponding to a thickness of about 0.34 nm, which is higher than that of the conventional organic or inorganic film.

As a general method of producing graphene, graphene having a large area and high quality on a metal substrate can be produced by chemical vapor deposition (CVD) (Chemical Vapor Deposition). In order to manufacture a sealing film using graphene, graphene must be separated and transferred onto a metal substrate. In the conventional process, a wet transfer method of etching a metal was used.

In such a conventional wet transfer process, defects, wrinkles, and the like are induced in the graphene, thereby adversely affecting the characteristics of the sealing film of the graphene. Further, in the wet transfer process, the metal substrate must be discarded after one use, which is not economical and requires a long etching time, which is not suitable for mass production. Moreover, environmental problems can also be caused through the metal etchant.

It is an object of the present invention to provide a method of manufacturing a graphene sealing film which can effectively block moisture and gas outside by using a dry transfer method of graphene.

Another object of the present invention is to provide a method of manufacturing an organic electronic device including the graphene encapsulation film.

In order to accomplish the object of the present invention, in a method of manufacturing a graphene sealing film according to embodiments of the present invention, a first graphene layer is formed on a base substrate. A first organic film is bonded onto a target substrate. The first graphene layer is mechanically peeled from the base substrate and transferred onto the first organic film.

In exemplary embodiments, the step of forming the first organic film on the target substrate may include coating a first organic film on the release paper, laminating the target substrate on the first organic film, And removing the release paper.

In exemplary embodiments, the step of laminating the target substrate on the first organic layer may be performed by vacuum laminating or roll laminating.

In the exemplary embodiments, the step of transferring the first graphene layer onto the first organic layer may include thermocompression bonding the base substrate and the target substrate on which the first graphene layer is formed .

In exemplary embodiments, the step of thermocompression bonding the base substrate and the target substrate may be performed within a pressure range of 10 kPa to 1 MPa and a temperature range of 100 ° C to 200 ° C.

In exemplary embodiments, the method includes forming a second graphene layer on the base substrate, bonding a second organic film on the first graphene layer, and bonding the second graphene layer to the base And mechanically peeling the substrate from the substrate and transferring the substrate on the second organic film.

In exemplary embodiments, the method may further include, after the step of transferring onto the second organic layer, removing the target substrate to form the first graphene layer, the first organic layer, And forming a graphene encapsulation layer including the first organic layer, the pinned layer, and the second organic layer.

In exemplary embodiments, the step of mechanically peeling the first graphene layer from the base substrate may include separating the base substrate and the target substrate using a peel device.

In exemplary embodiments, forming the first graphene layer on the base substrate includes forming a catalyst layer on the base substrate and growing the first graphene layer on the catalyst layer .

In exemplary embodiments, the step of growing the first graphene layer may be performed by a chemical vapor deposition process.

In exemplary embodiments, the first organic film may comprise an epoxy.

According to another aspect of the present invention, there is provided a method of manufacturing an organic electronic device including a graphene encapsulation layer, the method comprising: forming an organic light emitting device on a substrate; And a graphene encapsulating film covering the organic light emitting device is formed on the substrate. The step of forming the graphene sealing film may include the steps of forming a first graphene layer on the base substrate, bonding the first organic film on the target substrate, and mechanically peeling the first graphene layer from the base substrate, 1 organic film.

In exemplary embodiments, the method may further include forming a second graphene layer on the base substrate, bonding a second organic film on the first graphene layer, and mechanically peeling the second graphene layer from the base substrate And transferring the organic layer onto the second organic layer.

In exemplary embodiments, the method may further include forming a second graphene layer on the base substrate, bonding a second organic film on the first graphene layer, and mechanically peeling the second graphene layer from the base substrate And transferring the organic layer onto the second organic layer.

In exemplary embodiments, the step of mechanically peeling the first graphene layer from the base substrate may include separating the base substrate and the target substrate using a peel device.

According to exemplary embodiments, in the method of manufacturing a graphene sealing film, it is possible to perform a mechanical transfer without etching to re-grow a high-quality single-layer graphene repeatedly without damaging the metal substrate, It is possible to mass-produce graphene devices in an environmentally friendly manner.

However, the effects of the present invention are not limited to the above-mentioned effects, and may be variously expanded without departing from the spirit and scope of the present invention.

1 is a flow chart showing a method of manufacturing a graphene sealing film according to an embodiment of the present invention.
FIGS. 2 to 9 are perspective views showing a method of manufacturing a graphene sealing film according to exemplary embodiments. FIG.
10 to 12 are cross-sectional views illustrating a method of manufacturing an organic electronic device including a graphene encapsulating film according to exemplary embodiments.

For the embodiments of the invention disclosed herein, specific structural and functional descriptions are set forth for the purpose of describing an embodiment of the invention only, and it is to be understood that the embodiments of the invention may be practiced in various forms, The present invention should not be construed as limited to the embodiments described in Figs.

The present invention is capable of various modifications and various forms, and specific embodiments are illustrated in the drawings and described in detail in the text. It is to be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but on the contrary, is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

The terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms may be used for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.

It is to be understood that when an element is referred to as being "connected" or "connected" to another element, it may be directly connected or connected to the other element, . On the other hand, when an element is referred to as being "directly connected" or "directly connected" to another element, it should be understood that there are no other elements in between. Other expressions that describe the relationship between components, such as "between" and "between" or "neighboring to" and "directly adjacent to" should be interpreted as well.

The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In the present application, the terms "comprise", "having", and the like are intended to specify the presence of stated features, integers, steps, operations, elements, components, or combinations thereof, , Steps, operations, components, parts, or combinations thereof, as a matter of principle.

Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries should be construed as meaning consistent with meaning in the context of the relevant art and are not to be construed as ideal or overly formal in meaning unless expressly defined in the present application .

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The same reference numerals are used for the same constituent elements in the drawings and redundant explanations for the same constituent elements are omitted.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart showing a method of manufacturing a graphene sealing film according to exemplary embodiments. FIG. FIGS. 2 to 9 are perspective views showing a method of manufacturing a graphene sealing film according to exemplary embodiments. FIG.

1 to 9, a method of manufacturing a graphene sealing film according to exemplary embodiments includes forming a graphene layer by a chemical vapor deposition (CVD) process, and repeating a reproducible mechanical transfer process, And transferring the graphene layer onto the organic film.

First, a first graphene layer 120 is formed on a base substrate 100 (S100).

As shown in FIG. 2, the catalyst layer 110 may be formed on the base substrate 100. In the exemplary embodiments, the base substrate 100 may be a silicon substrate. Further, a silicon oxide layer (not shown) may be further formed on the base substrate 100.

The catalyst layer 110 may serve to help the carbon components combine with each other to form a hexagonal plate-like structure. For example, the catalyst layer 110 may be formed from a group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, One or more selected metals or alloys may be used.

In this embodiment, the catalyst layer 110 may include copper. Since copper has a relatively low solubility in carbon, it may be advantageous to form a large-area single layer of graphene.

Next, a first graphene layer 120 is formed on the catalyst layer 110. A catalyst layer 110 made of a metal is deposited on a base substrate 100 and then a base substrate 100 is loaded into a chamber of a chemical vapor deposition A large-area graphene monolayer can be formed. Therefore, a high-quality single-layered first graphene layer 120 having a low defect density can be formed over a large area with good uniformity on the copper catalyst layer 110.

Thereafter, the first organic layer 130 is bonded to the target substrate 200 (S200).

As shown in FIG. 3, the first organic layer 130 may be coated using a film coating method. The first organic layer 130 may include a substance having an adhesive property to the surface of the graphene. For example, the first organic layer 130 may be formed to include a high molecular material such as an epoxy. The first organic layer 130 may be coated to have a thickness ranging from 10 to 50 mu m.

The target substrate 200 can be, for example, a flexible substrate or a rigid substrate, specifically, a polyimide substrate, a glass substrate, or a silicon substrate.

In the exemplary embodiments, the first organic film 130 may be coated on the release paper 135 and then lapped with the target substrate 200.

At this time, the lapping process may be performed using vacuum lamination or roll lamination, and the release paper 135 may be removed from the target substrate 200 after the lapping process.

The lapping process may be performed at a temperature of at least 40 < 0 > C. On the other hand, the thermosetting polymer such as an epoxy material can be cured at a high temperature, so that the laminating process can be performed at a temperature lower than the curing initiation temperature of the polymer used for the first organic film 300.

Next, the first graphene layer 120 is mechanically peeled from the base substrate 100 and transferred onto the first organic layer 130 (S300).

4, the base substrate 100 on which the first graphene layer 120 is formed and the target substrate 200 on which the first organic layer 130 is formed are thermally bonded to each other.

Specifically, the thermocompression bonding process may be performed at a pressure ranging from 10 kPa to 1 MPa and a temperature range of 100 ° C to 200 ° C using a hot press. At this time, the epoxy material is cured for 30 minutes to 2 hours to improve the adhesion, so that the bonding force between the temporary substrate 200 and the base substrate 100 on which the first graphene layer 120 is formed can be maintained .

5, grips (not shown) of the mechanical separator are attached to one surface of the base substrate 100 and one surface of the target substrate 200 using an adhesive, and then the base (not shown) 100 and the target substrate 200 can be moved in directions opposite to each other. Accordingly, the first graphene layer 120 may be mechanically peeled off from the catalyst layer 110 and transferred to the first organic layer 120 at the same time.

The mechanical separator may be a 90 degree peel device or a 180 degree peel device, and the peeling process may be performed at a speed ranging from 0.01 m / s to 100 nm / s.

At this time, the binding energy between the first graphene layer 120 and the catalyst layer 110 may be smaller than the binding energy between the first graphene layer 120 and the first organic layer 130. Therefore, when the mechanical separator is loaded, the first graphene layer 120 having a low binding energy with the catalyst layer 110 is advantageously peeled from the catalyst layer 110 rather than the first organic layer 130, (110). ≪ / RTI >

The transferring process of the conventional graphene layer is carried out through a wet transfer process, and the wet transfer process causes defects such as wrinkles in the graphene, which adversely affects the characteristics of the graphene sealing film. On the other hand, since the graphene encapsulating film according to the exemplary embodiments is transferred through the dry transfer process, the above problem does not exist, and thus it is possible to have more improved characteristics.

6, a second organic layer 140 is formed on the entire surface of the first graphene layer 120 formed on the target substrate 200. Next, as shown in FIG. The method of forming the second organic film 140 is substantially the same as the method of forming the first organic film 130 described with reference to FIG. 3, and thus a detailed description thereof will be omitted.

7 to 9, after the second graphene layer 150 is formed on the base substrate 100, the second graphene layer 150 is mechanically peeled off from the base substrate 100, And transferred onto the organic film 140.

7, after the second graphene layer 150 is formed on the base substrate 100 from which the first graphene layer 120 is removed, the second substrate 140 having the second organic film 140 formed thereon ). The method of forming the second graphene layer 150 and the thermocompression step are substantially the same as the method of forming the first graphene layer 120 described with reference to FIG. 2 and the thermocompression method described with reference to FIG. 5, The description is omitted. At this time, the base substrate 100 may additionally be reused for graphene growth and transfer processes.

8, the second graphene layer 150 may be mechanically peeled off from the copper catalyst layer 110 and simultaneously transferred onto the target substrate 200 having the second organic film 140 formed thereon.

The transfer method of the second graphene layer 150 is similar to that of the first embodiment except that the second graphene layer 150 is transferred instead of the first graphene layer 120 and that the second organic film 140 is formed on the target substrate 200 5, the detailed description thereof will be omitted.

9, the target substrate 200 is removed and the first organic layer 130, the first graphene layer 120, the second organic layer 140, and the second graphene layer 150 are sequentially formed A graphene sealing film can be formed.

The second graphene layer 150 and the second organic layer 140 are formed on the first graphene layer 120 and the first organic layer 130. However, , Two or more alternately stacked organic films and a graphene layer may be further formed.

As described above, various advantages can be expected when the graphene sealing film is manufactured by using the dry transfer method. First, the dry transfer method can reduce the graphene bond and wrinkle unlike the wet transfer process, thereby enhancing the water and gas barrier properties of the graphene sealing film. Second, the metal substrate can be recycled by transferring the graphene without damaging the metal substrate used as the base substrate, unlike the case of using the wet transfer process. As a result, the base substrate can be recycled, and a large amount of graphene sealing film can be used in an economical and environmentally friendly manner.

10 to 12 are cross-sectional views illustrating a method of manufacturing an organic electronic device including a graphene encapsulating film according to exemplary embodiments.

10 and 11, a driving circuit portion 460 and an organic light emitting element 470 are formed on a base substrate 410 to form a display panel of an OLED display.

The driving circuit portion 460 may be formed to include at least two thin film transistors and at least one storage capacitor, and the thin film transistor may basically be formed to include a switching transistor T and a driving transistor (not shown) have.

The organic light emitting diode 470 may include a first electrode (hole injection electrode / anode) 472, an organic emission layer 474, and a second electrode (electron injection electrode / cathode) 476.

Specifically, the base substrate 410 may include a flexible substrate. The base substrate 410 may include a curved surface and may include a transparent insulating material suitable for supporting conductive patterns and layers to be laminated. A buffer layer 412 may be provided on the base substrate 410.

The switching transistor T may be formed to include a semiconductor pattern 420, a gate electrode 430, a source electrode 442, and a drain electrode 444. [ A gate insulating layer 422 may be interposed between the semiconductor pattern 420 and the gate electrode 440. The transistor may be a thin film transistor having a top-gate structure, or the transistor may be a thin film transistor having a bottom-gate structure.

An interlayer insulating film 432 is provided on the gate insulating film 422 and may be formed to cover the gate electrode 430. The interlayer insulating film may be formed to have a multi-layer structure including inorganic films. The inorganic film may be formed to include silicon oxide, silicon nitride, silicon oxynitride, silicon carbonitride, silicon oxycarbide, and the like.

The passivation layer 450 may be formed to cover the source electrode 442 and the drain electrode 444 and have a substantially flat upper surface and the passivation layer 450 may be formed to have an opening exposing the drain electrode 444 .

A first electrode 472 connected to the drain electrode 444 may be formed on the passivation layer 450. A pixel defining layer exposing the first electrode 472 may be further formed on the passivation layer 450. An organic light emitting layer 474 and a second electrode 476 may be sequentially formed on the first electrode 472.

Referring to FIG. 12, a graphene encapsulating film 500 covering the organic light emitting device 470 may be formed on a base substrate 410.

That is, a process similar to or similar to the process described with reference to FIGS. 1 to 9 is performed to form the first graphene layer 530, the first organic layer 540, the second graphene layer 550, A third graphene layer 570, and a third organic layer 580 are successively stacked on the first organic layer 560, the second organic layer 560, the third organic layer 570, and the third organic layer 580. Thereafter, the graphene sealing film 500 may be disposed to cover the organic light emitting device 470 formed on the base substrate 410.

The graphene encapsulation film 500 of the organic light emitting diode display 400 formed on the base substrate 410 can disperse the stress acting when the base substrate 110 is bent or curved, 470 to prevent oxygen or moisture from permeating.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention as defined in the appended claims. And changes may be made without departing from the spirit and scope of the invention.

The graphene encapsulation film described above can be applied to various fields in which a graphene encapsulation film is required. For example, organic-based electronic devices. In the case of organic transistors and organic light emitting devices, electronic devices must be protected from external moisture and gases in order to ensure reliable operation. By using this invention, a high-performance, low-cost, large-area graphene encapsulating film can be manufactured, thereby solving the problem of reliability and mass production of the organic electronic device

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined in the following claims. It can be understood that it is possible.

100: base substrate 110: catalyst layer
120: first graphene layer 130: first organic film
140: second organic film 150: second graphene layer
200: target substrate

Claims (15)

Forming a first graphene layer on the base substrate;
Bonding the first organic film to a target substrate; And
And mechanically peeling the first graphene layer from the base substrate and transferring the graphene layer onto the first organic layer. The method of claim 1, wherein forming the first organic layer on the target substrate comprises:
Coating a first organic film on the release paper;
Laminating the target substrate on the first organic layer; And
And removing the release paper. ≪ RTI ID = 0.0 > 15. < / RTI > [3] The method of claim 2, wherein the step of laminating the target substrate on the first organic layer is performed by vacuum laminating or roll laminating. The method of claim 1, wherein the step of transferring the first graphene layer onto the first organic film comprises thermocompression bonding the base substrate and the target substrate on which the first graphene layer is formed A method for producing a graphene sealing film. The method of claim 4, wherein the step of thermocompression bonding the base substrate and the target substrate is performed in a pressure range of 10 kPa to 1 MPa and a temperature range of 100 to 200 캜. The method according to claim 1,
Forming a second graphene layer on the base substrate;
Bonding the second organic film to the first graphene layer; And
Further comprising the step of mechanically peeling the second graphene layer from the base substrate and transferring the second graphene layer onto the second organic film. The method of claim 6, further comprising the step of removing the target substrate to form a graphene encapsulating layer including the first graphene layer, the first organic layer, the second graphene layer, and the second organic layer stacked on each other Wherein the graphene encapsulation layer is formed by a method comprising the steps of: The method of claim 1, further comprising mechanically peeling the first graphene layer from the base substrate, separating the base substrate and the target substrate using a peel device, A method for producing an encapsulating membrane. The method of claim 1, wherein forming the first graphene layer on the base substrate comprises:
Forming a catalyst layer on the base substrate; And
And growing the first graphene layer on the catalyst layer. 10. The method of claim 9, wherein the step of growing the first graphene layer is performed by a chemical vapor deposition process. The method of claim 1, wherein the first organic layer comprises an epoxy. Forming an organic light emitting element on a substrate;
And forming a graphene sealing film covering the organic light emitting device on the substrate,
The step of forming the graphene sealing film
Forming a first graphene layer on the base substrate;
Bonding the first organic film to a target substrate; And
And mechanically peeling the first graphene layer from the base substrate and transferring the first graphene layer onto the first organic layer. 13. The method of claim 12,
Forming a second graphene layer on the base substrate;
Bonding the second organic film to the first graphene layer; And
And mechanically peeling the second graphene layer from the base substrate and transferring the second graphene layer onto the second organic film. 14. The method of claim 13, further comprising the step of removing the target substrate to form a graphene encapsulating layer including the first graphene layer, the first organic layer, the second graphene layer, and the second organic layer stacked on each other Wherein the organic electronic device is a silicon wafer. The method of claim 12, wherein mechanically peeling the first graphene layer from the base substrate comprises separating the base substrate and the target substrate using a peel device. / RTI >

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